EP0082934A2 - Détecteur d'humidité et procédé de sa fabrication - Google Patents
Détecteur d'humidité et procédé de sa fabrication Download PDFInfo
- Publication number
- EP0082934A2 EP0082934A2 EP82109687A EP82109687A EP0082934A2 EP 0082934 A2 EP0082934 A2 EP 0082934A2 EP 82109687 A EP82109687 A EP 82109687A EP 82109687 A EP82109687 A EP 82109687A EP 0082934 A2 EP0082934 A2 EP 0082934A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- tantalum
- layer
- oxide layer
- tantalum oxide
- density
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
- G01N27/223—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance for determining moisture content, e.g. humidity
- G01N27/225—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance for determining moisture content, e.g. humidity by using hygroscopic materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/121—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid for determining moisture content, e.g. humidity, of the fluid
Definitions
- the invention relates to a moisture sensor with a thin layer of the oxide of high-resistance porous low density tantalum ("low density" tantalum) applied to a moisture-insensitive substrate and with at least two electrodes arranged at a distance from one another on the tantalum oxide layer, and to a method for producing one such a moisture sensor.
- low density tantalum porous low density tantalum
- a moisture sensor of this type is the subject of the older European patent application 81104405.6.
- one of the two electrodes is a base electrode, which is arranged between the substrate and the tantalum oxide layer.
- this base electrode is formed together with the tantalum oxide layer in that a layer made of the "low density” tantalum is only oxidized over part of its thickness, so that it is under the tantalum oxide layer part of the metallic "low density” tantalum remains, which forms the base electrode.
- This type of base electrode formation is possible with the "low density” tantalum specified in the main application, which has a specific resistance that reaches values of up to 40,000 ⁇ cm. With the density and porosity of the "low density” tantalum corresponding to this resistance value, controlled oxidation down to the desired depth is possible.
- the invention has for its object to develop the moisture sensor according to the main application so that it can be easily formed with a base electrode even when the tantalum oxide layer is formed from very high-resistance "low density" tantalum.
- valve metals are anodically oxidizable metals, which include in particular tantalum, aluminum and niobium.
- the metal of the base electrode is progressively oxidized from the surface, the oxidation depth being determined by the oxidation parameters. In this way, reliable control of the oxidation process is possible without the base electrode disappearing.
- the oxide layer formed from the metal of the base electrode has the additional advantage that it can serve as insulation from the required counter electrode. The counter electrode can therefore (particularly in the form of a cover electrode) be applied directly to the oxidized structure.
- tantalum is also used as the metal for the base electrode, but with a greater density than in the "low density" tantalum layer used for the formation of the moisture-sensitive tantalum oxide. It is then possible to dust the two layers practically in one operation in the same system, with only the sputtering parameters being set differently in order to achieve the desired different densities.
- the moisture-sensitive layer of the moisture sensor according to the invention can be produced from extremely porous tantalum oxide, it has a very high sensitivity.
- a further improvement makes it possible to considerably increase the response speed of the moisture sensor if it is equipped with a cover electrode which partially covers the tantalum oxide layer and which has cutouts through which the water vapor-containing medium can penetrate into the moisture-sensitive tantalum oxide layer. This is because only the areas of the tantalum oxide layer lying between the electrodes are active for the moisture measurement; the water vapor must therefore first penetrate the inactive areas below the cutouts in order to reach the active areas.
- the response speed of the moisture sensor is significantly increased in that the inactive areas of the tantalum oxide layer lying under the cutouts are removed.
- the inactive areas are preferably removed by plasma etching, the cover electrode being used as an etching mask.
- an etching protection layer 2 is applied to a substrate 1 made of glass or another translucent material (FIG. 2a).
- the etching protection layer 2 is required in particular if wet chemical etching with hydrofluoric acid is carried out in method step V, since hydrofluoric acid attacks glass.
- the etching protection layer 2 can consist of tantalum oxide Ta 2 0 5 and be formed by first sputtering a tantalum layer with a thickness of about 150 nm in vacuo onto the glass substrate 1, which has a thickness of 0.6 mm, for example, and then oxidizing it .
- the oxidation can be carried out in air at a temperature of about 450 ° C; it should last at least 5 hours, but preferably up to about 16 hours.
- the tantalum oxide layer obtained in this way has a thickness of approximately 300 nm.
- the layer 3 can consist of solid tantalum in the a modification or in the ⁇ modification.
- tantalum of the a modification has a density of 15.6 g / cm 3 and a specific resistance of 25 to 50 ⁇ cm
- tantalum of the ß modification has a density of 15.9 g / cm 3 and a specific resistance of 180 up to 220 ⁇ cm.
- bulk piece tantalum
- the "low density” tantalum is a special modification of tantalum which, like the a and ⁇ modifications mentioned above, is also only present in thin layers, but is different from these and thus from piece tantalum with regard to structure, density and specific resistance.
- the "low density” tantalum arises under certain conditions when sputtering (sputtering) tantalum in thin layers, whereby the sputter voltage, ie the acceleration voltage of the argon ions, has emerged as an essential parameter. With decreasing sputtering voltage, the structure of the tantalum in the thin layer becomes increasingly porous, and accordingly, the density decreases to values which 10 g / cm 3 and less can, wherein the p s ezifi- specific resistance assumes very high values.
- the tantalum of layers 3 and 4, which is not covered by the etching mask 5, is removed by wet chemical etching.
- a mixture of hydrofluoric and nitric acids can be used for this, which has the following composition:
- the moisture-sensitive layer of tantalum oxide Ta 2 0 5 is formed by anodic oxidation of the high-resistance porous tantalum of layer 4. Since the electrode connection 8 must not be oxidized, it is covered by an oxidation mask.
- the oxidation mask can again be formed photolithographically using photoresist in the manner specified above, preferably with a thickness of approximately 10 to 20 ⁇ m.
- the oxidation takes place, for example, by anodizing in aqueous electrolyte.
- aqueous electrolyte For example, a 0.01% citric acid can be used for this, the tantalum layers 3 and 4 being connected to the positive pole of the voltage source.
- the structure After removing the oxidation mask. the structure has the appearance shown in Figures 2f and 3b.
- Fig. 2f shows that the very porous and high-resistance tantalum of layer 4 is completely oxidized, while the denser tantalum of layer 3 is only oxidized to a certain depth of penetration, so that metallic tantalum is still present under the oxide layer. This is the result of the very different density of tantalum in layers 3 and 4.
- the oxidation takes place practically immediately over the entire thickness of the layer, so that it is in particular not possible to determine the depth of oxidation by Control oxidation conditions.
- the oxidation takes place progressively in the usual manner from the outside inwards as a function of the surface current and the anodization voltage, so that it is possible to control the depth of oxidation by adjusting these parameters.
- the structure formed in this way thus contains a comb-shaped metallic base electrode 10, which consists of the remaining metallic tantalum of the layer 3 and is electrically connected to the electrode connection 8, in which the metallic tantalum of the original layers 3 and 4 is still completely preserved.
- the base electrode 10 is covered with a tantalum oxide layer 11, which is produced by anodic oxidation of the denser tantalum Layer 3 was created.
- a tantalum oxide layer 12 which is formed by the complete anodic oxidation of the "low density" tantalum of the layer 4.
- the tantalum oxide layer 12 forms the actual moisture-sensitive layer of the moisture sensor.
- the tantalum oxide layer 12 Since the tantalum of layer 4 was extremely porous, the tantalum oxide layer 12 also has a very porous structure, with the result that it is particularly sensitive to moisture, with both the dielectric constant and the resistivity changing greatly depending on the moisture absorbed. Nevertheless, this porous tantalum oxide has the same long-term electrical stability and chemical resistance as normal tantalum oxide.
- step VII the "lift off" mask is formed.
- the comb structure obtained last (FIGS. 2f and 3b) is covered with a photoresist layer 13, which is then exposed through the glass substrate 1 (FIG. 2g).
- the comb structure previously obtained from the base electrode 10 and the oxide layers 11 and 12 forms the exposure mask.
- the exposed parts are removed, so that only the unexposed parts remain as a "lift off” mask 14 (FIGS. 2h and 3c).
- the "lift off” mask 14 has the shape of the comb structure and it covers the oxide layer 12, with the exception of a narrow area along the edges. This somewhat smaller width of the "lift off” mask 14 is the result of the scattering of the light at the edges of the comb structure serving as an exposure mask.
- the metal layers from which the cover electrode is to be formed are evaporated onto the entire surface of the structure obtained last.
- Gold is preferably used as the conductor material for the cover electrode.
- a chrome layer 15 is first vapor-deposited on the entire surface and this is then covered with a gold layer 16 by vapor deposition (FIG. 2i).
- titanium or tantalum can also be used for the adhesive layer.
- tantalum as an adhesive layer, it is advisable to insert a chrome layer between the tantalum layer and the gold layer.
- the top layer of the cover electrode can also consist of aluminum instead of gold.
- process step IX the "lift off” mask made of photoresist together with the chromium and gold above it is detached.
- the solvent acetone
- the structure thus obtained is shown in section in FIG. 2k and in plan view in FIG. 3d.
- a comb-shaped window 17 has been created in which the tantalum oxide layer 12 is exposed. Since the chromium and gold layers 15, 16 still cover the entire remaining surface of the substrate, the sections which are not required are removed by a subsequent etching process in method step X, so that the cover electrode 18 is given the final shape, which is shown in plan view in FIG. 3e is.
- the etching can be carried out in the same manner as before when the base electrode 10 was formed in process steps IV and V, by first forming an etching mask by exposing and developing a photoresist layer, then the chromium and gold layers on the not by the areas covered by the etching mask are removed by wet chemical etching and finally the etching mask is removed.
- etchants suitable for chrome and gold must be used; Examples of this are given in the main application.
- the cover electrode 18 is completely separated from the base electrode 10 by the tantalum oxide layers 11 and 12. It extends somewhat along the edges over the top of the moisture-sensitive tantalum oxide layer 12, which is otherwise exposed in the cutouts formed by the window 17. Due to the overlap is produced between the base electrode 10 and the D corner electrode 18 a certain mutual overlap, the advantageous for the sensitivity of the moisture sensor, as active for the moisture measurement of the tantalum oxide layer 12 is formed by between the electrodes 10 and 18 areas, which are designated in Fig. 2k with 12a.
- the response speed of the moisture sensor is determined by the time it takes for the water vapor to reach the active areas 12a (FIG. 2k). He must penetrate the inactive areas 12b, which are below the cutouts formed by the window 17.
- the response time of the moisture sensor is considerably shortened.
- a plasma etching in CF 4 with 0 2 addition is suitable as the etching method. If the top layer of the cover electrode 18 is made of gold or aluminum, the cover electrode 18 itself can serve as an etching mask, since these metals have a very low etching rate in the aforementioned plasma. No special etching mask is then required.
- the final moisture sensor After etching, the final moisture sensor has the structure shown in FIG.
- the water vapor can penetrate directly into the active regions 12a of the tantalum oxide layer 12.
- the 95% value of the output signal of the moisture sensor could be achieved in less than 1 second.
- anodically oxidizable metal in particular aluminum or niobium, can be used as the material for the base electrode 10 instead of tantalum.
- Such metals are known under the name "valve metals”.
- a base electrode made of a metal which has a greater density than the "low density” tantalum, from the oxide of which the moisture-sensitive layer is formed is also possible with other structures of the moisture sensor, for example with all in the Structures described in main filing. This measure is independent of the type, shape and manufacture of the counter electrode.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Non-Adjustable Resistors (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE3151630 | 1981-12-28 | ||
DE3151630A DE3151630C2 (de) | 1981-12-28 | 1981-12-28 | Feuchtigkeitsfühler und Verfahren zu seiner Herstellung |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0082934A2 true EP0082934A2 (fr) | 1983-07-06 |
EP0082934A3 EP0082934A3 (en) | 1983-10-05 |
EP0082934B1 EP0082934B1 (fr) | 1987-01-14 |
Family
ID=6149873
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP82109687A Expired EP0082934B1 (fr) | 1981-12-28 | 1982-10-20 | Détecteur d'humidité et procédé de sa fabrication |
Country Status (4)
Country | Link |
---|---|
US (1) | US4482882A (fr) |
EP (1) | EP0082934B1 (fr) |
JP (1) | JPS58165313A (fr) |
DE (1) | DE3151630C2 (fr) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2538115A1 (fr) * | 1982-12-21 | 1984-06-22 | Vaisala Oy | Detecteur d'humidite capacite et procede de fabrication |
WO1985004718A1 (fr) * | 1984-04-06 | 1985-10-24 | Fraunhofer-Gesellschaft Zur Förderung Der Angewand | Detecteur pour l'analyse de liquides |
Families Citing this family (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5269175A (en) * | 1984-04-06 | 1993-12-14 | Fraunhofer-Gesellschaft Zur Forderung Der Angewandten Forschung E.V. | Sensor for investigating liquids |
US4953387A (en) * | 1989-07-31 | 1990-09-04 | The Regents Of The University Of Michigan | Ultrathin-film gas detector |
ES2069784T3 (es) * | 1990-09-12 | 1995-05-16 | Endress Hauser Gmbh Co | Procedimiento para fabricar un sensor capacitivo de humedad. |
AT1469U1 (de) * | 1996-04-10 | 1997-05-26 | E & E Elektronik Gmbh | Verfahren zum ermitteln der absoluten luftfeuchtigkeit |
US6222376B1 (en) | 1999-01-16 | 2001-04-24 | Honeywell International Inc. | Capacitive moisture detector and method of making the same |
US6262877B1 (en) * | 1999-11-23 | 2001-07-17 | Intel Corporation | Low inductance high capacitance capacitor and method of making same |
US6489034B1 (en) | 2000-02-08 | 2002-12-03 | Gould Electronics Inc. | Method of forming chromium coated copper for printed circuit boards |
US6489035B1 (en) | 2000-02-08 | 2002-12-03 | Gould Electronics Inc. | Applying resistive layer onto copper |
US6622374B1 (en) | 2000-09-22 | 2003-09-23 | Gould Electronics Inc. | Resistor component with multiple layers of resistive material |
US6843899B2 (en) * | 2001-11-06 | 2005-01-18 | North Carolina State University | 2D/3D chemical sensors and methods of fabricating and operating the same |
US20060201247A1 (en) * | 2004-05-06 | 2006-09-14 | Honeywell International, Inc. | Relative humidity sensor enclosed with formed heating element |
US20120167392A1 (en) | 2010-12-30 | 2012-07-05 | Stmicroelectronics Pte. Ltd. | Razor with chemical and biological sensor |
DE102011054501A1 (de) * | 2011-10-14 | 2013-04-18 | Heinrich-Heine-Universität Düsseldorf | Sensor und Verfahren zum Herstellen eines Sensors |
US9019688B2 (en) | 2011-12-02 | 2015-04-28 | Stmicroelectronics Pte Ltd. | Capacitance trimming with an integrated heater |
US9027400B2 (en) * | 2011-12-02 | 2015-05-12 | Stmicroelectronics Pte Ltd. | Tunable humidity sensor with integrated heater |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2824609A1 (de) * | 1977-06-06 | 1978-12-07 | Matsushita Electric Ind Co Ltd | Vorrichtung zur feuchtigkeitsmessung durch kapazitaetsaenderung |
DE2938434B1 (de) * | 1979-09-22 | 1980-11-27 | Fraunhofer Ges Forschung | Kapazitiver Feuchtigkeitsfuehler und Verfahren zur Herstellung des Fuehlers |
EP0043001A1 (fr) * | 1980-06-27 | 1982-01-06 | Endress u. Hauser GmbH u.Co. | Jauge d'humidité et procédé pour sa fabrication |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5212497A (en) * | 1975-07-17 | 1977-01-31 | Osamu Sakurai | Metal oxide film moisture sensitive element |
GB1577724A (en) * | 1976-06-24 | 1980-10-29 | Molecular Controls Ltd | Humidity sensors |
DE2906813C2 (de) * | 1979-02-22 | 1982-06-03 | Robert Bosch Gmbh, 7000 Stuttgart | Elektronische Dünnschichtschaltung |
JPS57109319A (en) * | 1980-12-16 | 1982-07-07 | Yoshio Imai | Capacity type moisture sensor and method of producing same |
PL142901B1 (en) * | 1984-07-12 | 1987-12-31 | Lucja Gaczkowska | Apparatus for absorbing vapours and gases being emitted during glass etching processes |
-
1981
- 1981-12-28 DE DE3151630A patent/DE3151630C2/de not_active Expired
-
1982
- 1982-10-20 EP EP82109687A patent/EP0082934B1/fr not_active Expired
- 1982-11-30 US US06/445,656 patent/US4482882A/en not_active Expired - Lifetime
- 1982-12-27 JP JP57227189A patent/JPS58165313A/ja active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2824609A1 (de) * | 1977-06-06 | 1978-12-07 | Matsushita Electric Ind Co Ltd | Vorrichtung zur feuchtigkeitsmessung durch kapazitaetsaenderung |
DE2938434B1 (de) * | 1979-09-22 | 1980-11-27 | Fraunhofer Ges Forschung | Kapazitiver Feuchtigkeitsfuehler und Verfahren zur Herstellung des Fuehlers |
EP0043001A1 (fr) * | 1980-06-27 | 1982-01-06 | Endress u. Hauser GmbH u.Co. | Jauge d'humidité et procédé pour sa fabrication |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2538115A1 (fr) * | 1982-12-21 | 1984-06-22 | Vaisala Oy | Detecteur d'humidite capacite et procede de fabrication |
WO1985004718A1 (fr) * | 1984-04-06 | 1985-10-24 | Fraunhofer-Gesellschaft Zur Förderung Der Angewand | Detecteur pour l'analyse de liquides |
Also Published As
Publication number | Publication date |
---|---|
JPS58165313A (ja) | 1983-09-30 |
EP0082934B1 (fr) | 1987-01-14 |
EP0082934A3 (en) | 1983-10-05 |
DE3151630A1 (de) | 1983-07-14 |
DE3151630C2 (de) | 1986-07-03 |
US4482882A (en) | 1984-11-13 |
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